Acetic Acid → HCID 68130945、化合物

HRID 1287644ノート

反応式

HRID 1287644 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:23])[CH2:9][CH2:10][CH2:11][N:12]2[CH2:17][CH:16]=[C:15]([C:18]3OC=C[N:22]=3)[CH2:14][CH2:13]2)=[CH:4][CH:3]=1.[Cr](O)(O)(=O)=O.C(=O)([O-])[O-].[Na+].[Na+].Cl.[C:36](O)(=[O:38])[CH3:37]>CO.CCOCC>[O:38]1[CH:36]=[CH:37][C:18]([C:15]2[CH2:14][CH2:13][N:12]([CH2:11][CH2:10][CH2:9][C:8]([C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:7][CH:6]=3)=[O:23])[CH2:17][CH:16]=2)=[N:22]1

参加物

8

反応物 5

HCID 176Acetic Acid2 回HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 24425Chromic AcidHCID 21505599HCID 21505599、化合物

生成物 1

HCID 68130945HCID 68130945、化合物

試薬・触媒・溶媒 2

HCID 887Methanol触媒HCID 3283Diethyl Ether溶媒

実験手順

A 1.58 g. portion of 3,6-dihydro-α-(p-fluorophenyl)- 4-(2-oxazolyl)-1(2H)-pyridinebutanol, prepared as described in Example 15, in 45 ml. of acetic acid is stirred at room temperature. A 30 ml. portion of chromic acid in acetic acid is added dropwise. The mixture is stirred for 2 hours and allowed to stand overnight. A few drops of methanol are added, the mixture is poured into ice water and neutralized with sodium carbonate. The mixture is extracted with ether. The ether extract is dried over magnesium sulfate, filtered and evaporated yielding an oil which solidifies. This solid is dissolved in ether, alcoholic HCl is added and the mixture is filtered. The solid is slurried in acetone, filtered and recrystallized twice from ethanol, m.p. 178°-178.5° C.

後処理

  1. waitto stand overnight
  2. extractionThe mixture is extracted with ether
  3. extractionThe ether extract
  4. dry with materialis dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customyielding an oil which
  8. filtrationthe mixture is filtered
  9. filtrationfiltered
  10. customrecrystallized twice from ethanol, m.p. 178°-178.5° C.

出典と根拠

ORDレコード
ord-35dc9d50eab24fa0b440a732fed1ed25
出典データセット
uspto-grants-1976_10
特許番号
US03985754

反応ノート

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